홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Guanidine Hydrochloride → HCID 178513072, 화합물

HRID 492213
노트
인쇄 미리보기

반응식

HRID 492213 반응식
Cl.[NH2:2][C:3]([NH2:5])=[NH:4].C[O-].[Na+].Cl.[Cl:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[N:16]([C:20]1[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[N:23]=[CH:22][CH:21]=1)[CH:15]=[C:14]2[C:30](Cl)=[O:31].[K+].[Br-]>CO>[Cl:10][C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[N:16]([C:20]1[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[N:23]=[CH:22][CH:21]=1)[CH:15]=[C:14]2[C:30]([NH:4][C:3]([NH2:5])=[NH:2])=[O:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 5742Guanidine HydrochlorideHCID 253877Potassium BromideHCID 10942334Sodium MethoxideHCID 86596417HCID 86596417, 화합물

생성물 1

HCID 178513072HCID 178513072, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3.11 g (32.55 mmol) of guanidine hydrochloride are added to a solution of 1.76 g (32.55 mmol) of sodium methoxide in 60 cm3 of methanol at a temperature in the region of 20° C. under an argon atmosphere. After stirring at this temperature for 2 hours, the mixture is concentrated to dryness under reduced pressure (2.7 kPa). The residue is taken up in 60 cm3 of 1,2-dimethoxyethane, and 2.46 g (6.51 mmol) of 5-chloro-3-chlorocarbonyl-1-(quinolin-4-yl)-1H-indole hydrochloride are added. After stirring at the reflux temperature of the solvent for 2 hours, the reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa). The residue is triturated in 250 cm3 of water and the suspension is filtered and then dried. The residue is purified by chromatography on silica gel [eluent: dichloromethane/methanol (85/15 by volume)]. After the fractions containing the expected product have been concentrated to dryness under reduced pressure (2.7 kPa), 1.2 g of 5-chloro-3-guanidinocarbonyl-1-(quinolin-4-yl)-1H-indole are obtained in the form of a beige-colored powder melting at a temperature above 260° C. Mass spectrum (CI): m/e 363 (M+H)+)+ (base peak). IR spectrum (KBr): 3466; 3398; 3322; 1636; 1593; 1571; 1510; 1451; 1383; 1356; 1265; 1219; 881; 810; 792; 775 and 649 cm−1.

후처리

  1. concentrationthe mixture is concentrated to dryness under reduced pressure (2.7 kPa)
  2. stirringAfter stirring at the reflux temperature of the solvent for 2 hours
  3. concentrationthe reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa)
  4. customThe residue is triturated in 250 cm3 of water
  5. filtrationthe suspension is filtered
  6. customdried
  7. customThe residue is purified by chromatography on silica gel [eluent: dichloromethane/methanol (85/15 by volume)]
  8. additionAfter the fractions containing the expected product
  9. concentrationhave been concentrated to dryness under reduced pressure (2.7 kPa), 1.2 g of 5-chloro-3-guanidinocarbonyl-1-(quinolin-4-yl)-1H-indole
  10. customare obtained in the form of a beige-colored powder
  11. custommelting at a temperature above 260° C

출처 및 근거

ORD 기록
ord-74735bc2dc904a87872b11e888e5e7c0
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07531663B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트